CN107643309A - The analysis method of electrical steel surface coating - Google Patents
The analysis method of electrical steel surface coating Download PDFInfo
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- CN107643309A CN107643309A CN201710771123.9A CN201710771123A CN107643309A CN 107643309 A CN107643309 A CN 107643309A CN 201710771123 A CN201710771123 A CN 201710771123A CN 107643309 A CN107643309 A CN 107643309A
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- 238000000576 coating method Methods 0.000 title claims abstract description 95
- 239000011248 coating agent Substances 0.000 title claims abstract description 90
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 39
- 238000004458 analytical method Methods 0.000 title claims abstract description 26
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 79
- 238000005520 cutting process Methods 0.000 claims abstract description 65
- 230000005540 biological transmission Effects 0.000 claims abstract description 52
- 238000010894 electron beam technology Methods 0.000 claims abstract description 29
- 238000003466 welding Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 4
- 239000012043 crude product Substances 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052802 copper Inorganic materials 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 18
- 230000033228 biological regulation Effects 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 230000001360 synchronised effect Effects 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000007423 decrease Effects 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 92
- 229910000831 Steel Inorganic materials 0.000 description 5
- 238000000137 annealing Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 3
- 239000000391 magnesium silicate Substances 0.000 description 3
- 229960002366 magnesium silicate Drugs 0.000 description 3
- 229910052919 magnesium silicate Inorganic materials 0.000 description 3
- 235000019792 magnesium silicate Nutrition 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 229910000565 Non-oriented electrical steel Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000010813 municipal solid waste Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a kind of analysis method of electrical steel surface coating, belong to analysis method technical field.It comprises the following steps：1) pretreatment of electrical steel surface coating sample；2) coating sample surface is adjusted to electron beam and the common focus point of ion beam；3) metal deposit is carried out to coating sample surface；4) processing of digging pit is carried out using ion beam respectively to former and later two regions of coating sample；5) U-shaped cutting, extraction and welding are carried out to the coating sample after processing of digging pit；6) it is thinned and polishes.The analysis method of the present invention carries out being accurately positioned the transmission electron microscope sample for preparing electrical steel surface coating using focused ion beam, in conjunction with the microscopic appearance of conventional transmission electronic microscope photos electrical steel surface coating, solve the problems, such as that prior art analyzes electrical steel surface coating microscopic appearance.
Description
Technical field
The present invention relates to electrical steel surface coating, belongs to analysis method technical field, is specifically related to a kind of electrical sheet table
The analysis method of finishing coat.
Background technology
The face coat of electrical sheet is generally divided into two layers of bottom and insulating coating；Bottom be decarburizing annealing after in surface of steel plate
The vitreous magnesium-silicate bottom that the magnesia of coating generates with the silica Silicon-rich film reaction of surface of steel plate under the high temperature conditions
Layer；Insulating coating is the phosphate coating applied on high annealing magnesium silicate bottom.The silicon formed after electrical sheet high annealing
Sour magnesium bottom not only has insulating properties, corrosion resistance, and makes to produce tension reduction iron loss, the thinner stress of magnesium silicate crystal grain in steel
It is bigger.Also there are some researches prove can make it be changed domain structure by certain tension, improve magnetic using special insulation coating
Property, so as to reduce the loss of silicon steel sheet Unit Weight and reduce the magnetostriction of silicon steel sheet.Insulating coating should be able to resistance to insulated paint, transformation
The erosion of device oil, lubricant etc., tack is good, should be able to withstand stress relief annealing, and stress relief annealing is front and rear to survey steel
The insulating coating resistance minimum value of plate can meet user's requirement.As can be seen that the face coat quality of electrical sheet not only influences electricity
The magnetic property of work steel, and have large effect to performance.
The research worker of electrical sheet has been carried out greatly to the insulating properties and insulating coating adhesive force of electrical steel coatings at present
Quantifier elimination.Pass through established thick coating attachment model and electron probe microanalyser (EPMA), glow discharge spectrometry
(GDS), analyze and have studied non-oriented electrical steel insulating coating and peel off front and rear pattern and composition.It is another to there is researcher to be sent out using field
SEM (FE-SEM) is penetrated to observe the coating layer thickness of non-oriented electrical steel.Research finds method for making sample pair
Image quality plays a key effect.Because coating is thin (about 1.0 μm), traditional metallographic Ginding process can not clear accurate observation
To real coating layer thickness.After low-temperature brittle fracture and metal spraying processing, with regard to the clearly microcosmic charge pattern of coating section can be obtained.Due to
It is to be observed using field emission scanning electron microscope, so being only capable of obtaining the surface microscopic charge pattern of coating section, and can not obtains
Obtain the architectural feature of coating cross sections.
At present, there is certain deficiency in the coating for analyzing electrical sheet, main as follows：
1) ESEM or electron probe are only capable of observing the pattern and micro-area composition of coating, and as the phase structure of coating
Characteristic information can not but obtain.
2) because ESEM or electron probe resolution capability Relative Transmission Electronic Speculum are low, therefore the height of coating can not be observed
X rays topographs are differentiated, and electrical steel coatings are typically made up of several parts, pattern and structure are different, and these information can not obtain.
3) country not for the coating method for preparing transmission electron microscopy of electrical sheet, leads to not use transmission electron microscope observing at present
Electrical steel coatings.
Periodical《Metallurgical analysis》, 2015,35 (10)：14-18, disclose the focused ion beam of ferrous materials complex inclusion
Positioning processing and structural characterization, mainly describe and prepare complex inclusion using focused ion beam accurate positioning function, positioning
Transmission electron microscope section sample, a variety of thing phase morphologies of whole field trash are presented to greatest extent, in conjunction with the face point of energy disperse spectroscopy
The crystal structure analysis technology of analysis function and projection Electronic Speculum is comprehensively characterized to complex inclusion.By to field trash into
Analysis and the demarcation of thing phase diffraction pattern, finally give the thing phase composition of complex inclusion.
At present there has been no focused ion beam accurate positioning function is utilized, the transmission electricity of electrical steel surface coating is prepared in positioning
Mirror section sample.
The content of the invention
To achieve the above object, the invention discloses a kind of analysis method of electrical steel surface coating.The analysis method is
Carry out being accurately positioned the transmission electron microscope sample for preparing electrical steel surface coating using focused ion beam, in conjunction with conventional transmission electricity
Mirror analyzes the microscopic appearance of electrical steel surface coating, and it comprises the following steps：
1) pretreatment of electrical steel surface coating sample；
2) coating sample surface is adjusted to electron beam and the common focus point of ion beam；
3) gas aggradation is carried out to coating sample surface；
4) processing of digging pit is carried out using ion beam respectively to former and later two regions of coating sample；
5) U-shaped cutting, extraction and welding are carried out to the coating sample after processing of digging pit；
6) it is thinned and polishes；
7) transmission electron microscope observing is used；
The step 5) comprises the following steps：
51) control electron beam vertical with specimen surface, regulation coating sample surface is burnt in the copolymerization of electron beam and ion beam
Point, U-shaped cutting is carried out to the coating sample after processing of digging pit, and the one side for retaining coating sample is connected with matrix；
52) the sophisticated coating sample with after U-shaped cutting of nano-machine hand is welded together using ion beam；
53) continuing cutting coating sample makes it be separated with matrix, is taken the coating sample cut using nano-machine hand
Go out, obtain the crude product of transmission electron microscope sample；
54) welding position for adjusting the special copper mesh of transmission electron microscope places it in electron beam and ion beam Synchronous center,
The tip of regulation nano-machine hand makes it close to the welding position of copper mesh, using ion beam by the crude product of transmission electron microscope sample with
Copper mesh welds together；
55) tip of nano-machine hand is separated with the crude product of transmission electron microscope sample using ion beam.
Further, the step 6) comprises the following steps：
61) surface of the crude product of transmission electron microscope sample is adjusted to electron beam and the common focus point of ion beam；
62) the crude product constantly cutting to transmission electron microscope sample is thinned, and to electron beam it was observed that product is transparent, stops cutting
Cut, that is, complete the preparation of transmission electron microscope sample.
Yet further, in the step 62), cutting is thinned and carried out as follows：
621) the thinned parameter of cutting is arranged to：Sample stage is tilted ± 6 °, the crude product of transmission electron microscope sample is carried out
Cutting is thinned, and the flat shape of cutting is square, and cutting width is 1~2 μm, and depth of cut is 10~30 μm, controls ion beam
Flow for 2~4nA；
622) the thinned parameter of cutting is arranged to：Sample stage is tilted ± 4 °, the flat shape of cutting is square, and cutting is wide
Spend for 1~1.5 μm, depth of cut is 10~30 μm, and it is 1~2nA to control ion beam current；
623) the thinned parameter of cutting is arranged to：Sample stage is tilted ± 2 °, the flat shape of cutting is square, and cutting is wide
Spend for 0.5~1 μm, depth of cut is 10~30 μm, and it is 50~300pA to control ion beam current.
Further, in the step 4), the flat shape digged pit is trapezoidal, and trapezoidal height is 10~30 μm, along ladder
Shape long side starts to cut, and terminates to cut with trapezoidal short side, and depth of cut is 10~30 μm.
Further, in the step 4), ensure that ion beam is vertical with specimen surface, control the ion beam accelerating voltage to be
20~30kV, ion beam current are ＞ 15nA, and depth of cut is 10~30 μm.
Further, in the step 51), depth of cut is 2~5 μm, and ion beam accelerating voltage is 20~30kV, from
Beamlet stream is 1~4nA.
Further, in the step 53), continue depth of cut be 2~5 μm, ion beam accelerating voltage be 20~
30kV, ion beam current be 1~4nA, and regulation sample stage makes it decline 0.05~0.10mm, will have been cut using nano-machine hand
Coating sample takes out, then nano-machine hand adjustment is whole to the position that Electronic Speculum operating distance is 4.5~5.0mm.
Further, in the step 54), adjustment sample stage makes Electronic Speculum operating distance>10mm, then adjust transmission electron microscope
The position of special copper mesh and sample stage, the welding position of the special copper mesh of transmission electron microscope is set to be placed in electron beam and ion beam Synchronous
Center.
Beneficial effect：
The present invention has been successfully prepared the transmission electron microscope sample of electrical steel surface coating using focused ion beam, not only makes up
The problem of prior art analysis electrical steel surface coating microscopic appearance, and the analysis method of the present invention may also be combined with power spectrum and
Electronic diffraction etc. further obtains more information of electrical steel surface coating.
Brief description of the drawings
Fig. 1 is electron beam and ion beam common focus point schematic diagram in embodiment；
Fig. 2 is the planar structure schematic diagram of the sampling under embodiment intermediate ion beam observation visual angle；
Fig. 3 is the planar structure schematic diagram of the sampling under embodiment intermediate ion beam observation visual angle；
Fig. 4 is sample and the planar structure schematic diagram of copper mesh welding under embodiment intermediate ion beam observation visual angle；
Fig. 5 is the electrical steel coatings microscopic appearance that transmission electron microscope observing is used in embodiment；
Wherein, Fig. 2 is that ion beam is vertical with specimen surface, and Fig. 3 and Fig. 4 are that electron beam is vertical with sample surfaces, and in figure
Label is as follows：
Electrical steel surface coating sample 1, sample stage 2, common focus point 3, transmission electron microscope sample 4, region 5 of digging pit, area of digging pit
Domain 6, cutting zone 7, cutting zone 8, cutting zone 9, nano-machine hand 10, copper mesh 11.
Embodiment
The embodiment of the present invention carries out preparing transmission electron microscope using the AURIGA double-beam systems of Zeiss to electrical steel surface coating
Sample, the transmission electron microscope sample are JEM-2100F Flied emission transmission electron microscopes.
Present embodiment discloses a kind of analysis method of electrical steel surface coating, the analysis method is using focused ion beam
Carry out being accurately positioned the transmission electron microscope sample for preparing electrical steel surface coating, electrical sheet table is analyzed in conjunction with conventional analytical instruments
The microscopic appearance of finishing coat, it comprises the following steps：
1) pretreatment of electrical steel surface coating sample：It is specific be by sample cut growth × a width of 10 × 10mm, and
The pollutant of specimen surface is purged using instrument is cleaned by ultrasonic, dried up specimen surface after having cleaned；
2) coating sample surface is adjusted to electron beam and the common focus point of ion beam：Detailed process is that the step 1) is pre-
Sample after processing, electrical steel surface coating sample 1 as shown in Figure 1 load focused ion beam SEM two-beam system
In the sample stage of system, sample stage 2 as shown in Figure 1, sample is set then to control electronics accelerate (beamacceleration) close proximity to sample edge of table
Voltage is 5kV, and ion beam accelerating voltage is 30kV, continues sample stage tilting to 54 ° that (the present embodiment is preferably tilted to the left, such as
Shown in Fig. 1), adjustment Electronic Speculum operating distance is 5.1mm, specimen surface is placed in the common focus point of electron beam and ion beam, such as Fig. 1
Shown common focus point 3, the common focus point are also the position for taking transmission electron microscope sample.
3) gas aggradation is carried out to coating sample surface：Before the deposition, first using gas injection system (GIS) in sample
Spatial induction deposits, and creates vacuum environment, and concrete operations are that first the gas in gas injection system (GIS) is preheated 0.5 hour,
Then stretch into gas syringe needle to specimen surface to be deflated, control time 300s, induction and deposition takes coating sample table after terminating
Face length × a width of 20 × 2 μm region carry out Pt depositions, it is 200pA to control ion beam current.
4) processing of digging pit is carried out using ion beam respectively in former and later two regions of coating sample：As shown in Fig. 2 region 5
It is the planar structure schematic diagrams digged pit with 6, and the flat shape preferably digged pit is trapezoidal, trapezoidal height is 20 μm of (trapezoidal length
The distance between side and short side), start to cut along trapezoidal long side using ion beam, end side is trapezoidal short side, ensure from
Beamlet is vertical with specimen surface, and it is 30kV to control ion beam accelerating voltage, and ion beam current 16nA, depth of cut is 20 μm；
In addition, in above-mentioned cutting, it is necessary to monitored in real time to cutting process, and select large scale diaphragm and high line
Pattern is observed.
5) U-shaped cutting, extraction and welding are carried out to the coating sample after processing of digging pit：
The step 5) comprises the following steps：
51) control electron beam vertical with specimen surface, regulation coating sample surface is burnt in the copolymerization of electron beam and ion beam
Point, U-shaped cutting is carried out to the coating sample after processing of digging pit, and the one side for retaining coating sample is connected with matrix：Specific mistake
Sample stage is is tilted to 0 ° by journey first, i.e., electron beam is vertical with specimen surface, and adjustment Electronic Speculum operating distance is 5.1mm, makes painting
Layer specimen surface is in electron beam and the common focus point of ion beam, then the part in the region 7 and 8 shown in cutting drawing 3, the present embodiment are excellent
Favored area 7 and the flat shape in region 8 are square, square width for 0.5 μm the distance between (two side), control ion beam
Accelerating potential is 30kV, and ion beam current 2nA, depth of cut is 2 μm；Meanwhile need to carry out in fact cutting process in cutting
When monitor, once find cut through sample once need stop cut, change sample.
52) the sophisticated coating sample with after U-shaped cutting of nano-machine hand 10 is welded together using ion beam：Similarly
Using GIS to specimen surface induction and deposition, then adjust the tip of nano-machine hand 10 and make it close to sample, as shown in figure 3, will receive
Rice manipulator 10 is placed in directly over sample left end, and it is 50pA to control ion beam current, by the sophisticated and U-shaped cutting of nano-machine hand 10
Coating sample afterwards welds together.
53) continuing cutting coating sample makes it be separated with matrix, the coating sample that will have been cut using nano-machine hand 10
Take out, obtain the crude product of transmission electron microscope sample：Continue to cut the region 9 shown in Fig. 3, the flat shape in region 9 is
Square, square width is 0.5 μm, and it is 30kV to control ion beam accelerating voltage, and ion beam current 2nA, depth of cut is 2 μm；
Similarly, need to monitor cutting process in real time in cutting, need to stop cutting once finding to cut through sample, change examination
Sample.Then sample stage is declined 0.05mm, taken out the coating sample cut using nano-machine hand 10, then by nano-machine
Hand 10 is promoted to the position that Electronic Speculum operating distance is 4.8mm.
54) welding position for adjusting the special copper mesh 11 of transmission electron microscope is placed it in electron beam and ion beam Synchronous
The heart, the tip of regulation nano-machine hand 10 make it close to the welding position of copper mesh 11, using ion beam by transmission electron microscope sample
Crude product welds together with copper mesh 11：As shown in figure 4, make sample stage decline 5mm, by the special copper mesh 11 of transmission electron microscope rotate to
Current location, rise sample stage to common focus point, then adjust the tip of nano-machine hand 10 to make it close to the weld part of copper mesh 11
Position, specimen surface is deflated using GIS, controls ion beam current to be welded on the crude product of transmission electron microscope sample with copper mesh for 50pA
Together.
55) tip of nano-machine hand is separated with the crude product of transmission electron microscope sample using ion beam：Control ion beam
Flow for 2nA, until the tip of nano-machine hand and the crude product of transmission electron microscope sample are cut off.
6) it is thinned and polishes：
The step 6) comprises the following steps：
61) surface of the crude product of transmission electron microscope sample is adjusted to electron beam and the common focus point of ion beam：It is specifically
Sample stage is tilted to 54 ° (the present embodiment is preferably tilted to the left), adjustment Electronic Speculum operating distance is 5.1mm, puts specimen surface
In electron beam and the common focus point of ion beam；
62) the crude product constantly cutting to transmission electron microscope sample is thinned, and to electron beam it was observed that product is transparent, stops cutting
Cut, that is, complete the preparation of transmission electron microscope sample：
Specific process is preferably three times, to cut thinned parameter for the first time and be arranged to for the thinned number of cutting：By sample
Sample platform tilts ± 6 °, and cutting is carried out to the crude product of transmission electron microscope sample and is thinned, the flat shape of cutting is square, cutting width
For 2 μm, depth of cut is 20 μm, and it is 2nA to control ion beam current；Second of thinned parameter of cutting is arranged to：Sample stage is inclined
Tiltedly ± 4 °, the flat shape of cutting is square, and cutting width is 1.5 μm, and depth of cut is 20 μm, and it is 1nA to control ion beam current；
Third time is cut thinned parameter and is arranged to：Sample stage is tilted ± 2 °, the flat shape of cutting is square, and cutting width is 1 μ
M, depth of cut are 15 μm, and it is 100pA to control ion beam current, meanwhile, need to carry out in real time cutting process in above-mentioned cutting
Monitoring, and electron-beam voltage is adjusted to 20kV, and sample transparency is observed under electron beam, once sample be thinned to it is transparent if
Cutting stops.
7) the projection electron microscopic sample of above-mentioned preparation is placed in transmission electron microscope and observed, obtained electrical sheet as shown in Figure 5 and apply
The microscopic appearance of layer.
Claims (8)
1. a kind of analysis method of electrical steel surface coating, the analysis method is to be accurately positioned and made using focused ion beam
It is standby go out electrical steel surface coating transmission electron microscope sample, then observe under transmission electron microscope the microscopic appearance of electrical steel surface coating,
It is characterized in that：It comprises the following steps：
1) pretreatment of electrical steel surface coating sample；
2) coating sample surface is adjusted to electron beam and the common focus point of ion beam；
3) gas aggradation is carried out to coating sample surface；
4) processing of digging pit is carried out using ion beam respectively to former and later two regions of coating sample；
5) U-shaped cutting, extraction and welding are carried out to the coating sample after processing of digging pit；
6) it is thinned and polishes；
7) transmission electron microscope observing is used；
The step 5) comprises the following steps：
51) control electron beam vertical with specimen surface, adjust coating sample surface in electron beam and the common focus point of ion beam, it is right
The coating sample digged pit after handling carries out U-shaped cutting, and the one side for retaining coating sample is connected with matrix；
52) the sophisticated coating sample with after U-shaped cutting of nano-machine hand is welded together using ion beam；
53) continuing cutting coating sample makes it be separated with matrix, takes out the coating sample cut using nano-machine hand, obtains
To the crude product of transmission electron microscope sample；
54) welding position for adjusting the special copper mesh of transmission electron microscope places it in electron beam and ion beam Synchronous center, adjusts
The tip of nano-machine hand makes it close to the welding position of copper mesh, using ion beam by the crude product and copper mesh of transmission electron microscope sample
Weld together；
55) tip of nano-machine hand is separated with the crude product of transmission electron microscope sample using ion beam.
2. the analysis method of electrical steel surface coating according to claim 1, it is characterised in that：The step 6) includes as follows
Step：
61) surface of the crude product of transmission electron microscope sample is adjusted to electron beam and the common focus point of ion beam；
62) the crude product constantly cutting to transmission electron microscope sample is thinned, and to electron beam it was observed that product is transparent, stops cutting, i.e.,
Complete the preparation of transmission electron microscope sample.
3. the analysis method of electrical steel surface coating according to claim 2, it is characterised in that：In the step 62), cutting
It is thinned and carries out as follows：
621) the thinned parameter of cutting is arranged to：Sample stage is tilted ± 6 °, the crude product of transmission electron microscope sample is cut
It is thinned, the flat shape of cutting is square, and cutting width is 1~2 μm, and depth of cut is 10~30 μm, and it is 2 to control ion beam current
~4nA；
622) the thinned parameter of cutting is arranged to：Sample stage is tilted ± 4 °, the flat shape of cutting is square, and cutting width is
1~1.5 μm, depth of cut is 10~30 μm, and it is 1~2nA to control ion beam current；
623) the thinned parameter of cutting is arranged to：Sample stage is tilted ± 2 °, the flat shape of cutting is square, and cutting width is
0.5~1 μm, depth of cut is 10~30 μm, and it is 50~300pA to control ion beam current.
4. the analysis method of electrical steel surface coating according to claim 1, it is characterised in that：In the step 4), dig pit
Flat shape to be trapezoidal, trapezoidal height is 10~30 μm, starts to cut along trapezoidal long side, terminates to cut with trapezoidal short side, cut
Depth is cut as 10~30 μm.
5. the analysis method of electrical steel surface coating according to claim 4, it is characterised in that：In the step 4), ensure
Ion beam is vertical with specimen surface, and it is 20~30kV to control ion beam accelerating voltage, and ion beam current is ＞ 15nA, and depth of cut is
10~30 μm.
6. the analysis method of electrical steel surface coating according to claim 1, it is characterised in that：In the step 51), cutting
Depth is 2~5 μm, and ion beam accelerating voltage is 20~30kV, and ion beam current is 1~4nA.
7. the analysis method of electrical steel surface coating according to claim 1, it is characterised in that：In the step 53), continue
Depth of cut is 2~5 μm, and ion beam accelerating voltage is 20~30kV, and ion beam current is 1~4nA, and regulation sample stage makes its decline
0.05~0.10mm, the coating sample cut is taken out using nano-machine hand, then nano-machine hand adjustment is whole to Electronic Speculum work
Make the position that distance is 4.5~5.0mm.
8. the analysis method of electrical steel surface coating according to claim 1, it is characterised in that：In the step 54), adjustment
Sample stage makes Electronic Speculum operating distance>10mm, then the position of the special copper mesh of transmission electron microscope and sample stage is adjusted, make transmission electron microscope special
The welding position of copper mesh is placed in electron beam and ion beam Synchronous center.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710771123.9A CN107643309B (en) | 2017-08-31 | 2017-08-31 | Analysis method of electrical steel surface coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710771123.9A CN107643309B (en) | 2017-08-31 | 2017-08-31 | Analysis method of electrical steel surface coating |
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| Publication Number | Publication Date |
|---|---|
| CN107643309A true CN107643309A (en) | 2018-01-30 |
| CN107643309B CN107643309B (en) | 2020-04-07 |
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| CN112444435A (en) * | 2020-11-20 | 2021-03-05 | 国标（北京）检验认证有限公司 | Preparation method of block material planar transmission electron microscope sample |
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| CN115326503A (en) * | 2022-07-25 | 2022-11-11 | 武汉钢铁有限公司 | A kind of preparation method of rust layer cross-section sample |
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